HPLC-MS/MS法测定人血浆中乌苯美司浓度

目的建立高效液相色谱-串联质谱(HPLC-MS/MS)法测定人血浆中乌苯美司浓度。方法采用API3000型HPLC-MS/MS液质联用系统,Ultimate C18分析柱(50mm×4.6mm,5μm),流动相为甲醇-水-甲酸(70∶30∶0.05,V/V/V),流速为0.2mL/min,格拉司琼作为内标。样品经过固相萃取后浓缩进样,多反应离子检测模式,正离子扫描,离子源为ESI源。结果检测乌苯美司的线性范围为0.4～4000ng/mL,最低定量限为0.4ng/mL。批内精密度和批间精密度均小于6%。结论本法具有快速简便、灵敏准确的特点,可满足乌苯美司临床药物浓度测定的需要。     

LC-MS法测定大鼠血浆中EXH-1626的浓度

目的:建立测定大鼠血浆中EXH-1626浓度的液相色谱-质谱(LC-MS)方法?方法:大鼠血浆样品中加入内标卡马西平,经蛋白沉淀剂(甲醇∶5%硫酸锌溶液 = 70∶30,V/V)沉淀血浆蛋白后取上清液5 μl进行LC-MS测定?色谱条件:色谱柱为汉邦ODS C18柱(5 μm,150 mm × 4.6 mm),流动相为乙腈∶10 mmol/L醋酸铵水溶液(用乙酸调pH至3)70∶30,流速为0.6 ml/min,柱温30℃;质谱条件:采用电喷雾离子化(ESI)方式,以选择性离子监测(SIM)方式检测,EXH-1626和内标选择检测离子的质荷比(m/z)分别为453.3([M+H]+)和274.3([M+H]+)?结果:大鼠血浆中EXH-1626在5~10 000 ng/ml内线性关系良好(r = 0.999 7),最低定量限(LOQ)为5 ng/ml,由低到高(10?100?1 000和10 000 ng/ml)4个浓度的日内和日间精密度RSD均< 10%,绝对回收率均> 70%,相对回收率90%~110%?结论:该方法快速?准确,灵敏度高,操作简便,适用于EXH-1626血药浓度测定及其非临床药代动力学研究?     

盐酸帕洛诺司琼、胃复安、地塞米松联合应用预防妇科腹腔镜术后恶心呕吐的临床研究

目的探讨盐酸帕洛诺司琼、地塞米松、胃复安联合应用预防妇科腹腔镜手术后恶心呕吐的临床效果。方法选择ASAⅠ~Ⅱ级,拟在全身麻醉下行择期妇科腹腔镜手术的患者250例,随机分为A、B、C、D、E组,每组50例。A组术前30 min静滴胃复安10 mg,麻醉诱导前10 min静注盐酸帕洛诺司琼0.075 mg+地塞米松5 mg;B组麻醉诱导前10 min静注盐酸帕洛诺司琼0.075 mg;C组术前30 min静滴胃复安10 mg,麻醉诱导前10 min静注盐酸帕洛诺司琼0.075 mg;D组麻醉诱导前10 min静注盐酸帕洛诺司琼0.075 mg+地塞米松5 mg;E组为空白组,于麻醉诱导前10 min静脉注射生理盐水10 m L。观察患者手术后24 h内恶心呕吐的发生情况。结果 A、B、C、D、E组术后恶心呕吐总发生率分别为16.0%(8/50)、56.0%(28/50)、48.0%(24/50)、42.0%(21/50)和78.0%(39/50)。术后各组恶心呕吐等级比较,差异有统计学意义(P0.05)。其中A组恶心呕吐程度明显低于B、C或E组(P0.05),C、D组恶心呕吐程度明显低于E组(P0.05)。B、C、D组组间比较,差异无统计学意义(P0.05)。结论盐酸帕洛诺司琼联合胃复安、地塞米松在预防妇科腹腔镜术后恶心呕吐的效果优于单纯应用盐酸帕洛诺司琼或盐酸帕洛诺司琼分别复合地塞米松和胃复安。     

RPLC-ESI/MS法测定人血浆中阿普唑仑及其代谢产物的浓度

目的 建立RPLC-ESI/MS法测定人血浆中阿普唑仑及其代谢产物浓度的方法.方法 以地西泮为内标物;色谱柱:Agilent Zorbax SB C18柱(2.1 mm×30 mm,3.5 μm),流动相为10 mol/L乙酰胺-乙腈(2∶8),流速为0.2 ml/min,柱温30℃,进样量10μl;质谱条件为电喷雾电离源(ESI),检测方式为正离子电离、多离子反应监测(MRM).结果 阿普唑仑、α-羟基阿普唑仑和4-羟基阿普唑仑在0.5～50 ng/ml血浆浓度范围内线性关系良好(r=0.9996,r=0.9997,r=0.9994;n=7);批内和批间精密度均低于5%;最低检测限为0.5 ng/ml.结论 该方法灵敏、准确可用于临床上阿普唑仑及α-羟基阿普唑仑和4-羟基阿普唑仑的药代动力学研究.     

反相高效液相色谱法测定盐酸帕洛诺司琼注射液的含量

目的 建立盐酸帕洛诺司琼注射液含量测定的高效液相色谱方法.方法 采用Alltima C18色谱柱(4.6 mm&#215;250 mm,5μm),以0.02 mol&#183;L-1磷酸二氢钠溶液(含0.25%的三乙胺与0.01 mol&#183;L-1己烷磺酸钠,用磷酸调节pH值至3.0)-乙腈(40∶60)为流动相;检测波长为254 nm,流速为1.5 mL&#183;min-1.结果 线性范围为10.3～103.1 mg&#183;L-1,r=0.999 9;平均回收率为100.4%,RSD为0.95%(n=9).结论 本方法简便、可靠,可用于盐酸帕洛诺司琼注射液的含量测定.     

高效液相色谱-质谱-质谱联用法测定Beagle狗血浆中石杉碱甲

目的:建立狗血浆中石杉碱甲的液质联用测定法.方法:血浆样品经液液萃取,用高效液相色谱-质谱-质谱联用法检测.色谱柱为Nucleocil ODS柱,50×2.0 mm I.D.,5 μm,流动相为乙腈-甲醇-水-甲酸(20∶40∶40∶0.1,v/v).采用多反应监测,用于定量的离子为m/z 243→210(石杉碱甲)和m/z 257→226(内标N-甲基石杉碱甲).结果:线性范围为0.1～12 ng/ml,最低定量浓度为0.1 ng/ml,可以检测到Beagle狗静注和口服100 μg石杉碱甲后12 h的血药浓度.结论:该方法灵敏度高,简便快速,可用于药代动力学研究.     

帕洛诺司琼预防妇科腹腔镜手术后恶心呕吐的临床研究

目的观察帕洛诺司琼预防妇科腹腔镜手术后恶心呕吐的效果。方法择期全麻下行妇科腹腔镜手术的患者60例,随机分入帕洛诺司琼组(P组),昂丹司琼+地塞米松(D组),每组30例。麻醉诱导前各组分别静脉注射帕洛诺司琼0.25mg/10m(lP组),昂丹司琼4mg+地塞米松8m(gD组)。记录术后0～6h,6～12h,12～24h,24～48h四个时间段患者恶心呕吐的情况及完全缓解率(Complete Response Rate,CRR)。结果两组的术后6h、12h、24h和48h的CRR比较(P组vsD组):100%vs86.7%(P>0.05),100%vs66.7%(P<0.05),96.7%vs50%(P<0.05),83.3%vs50%(P<0.05)。各个观察时段内,P组恶心呕吐的发生率较D组少。结论与昂丹司琼复合地塞米松比较,帕洛诺司琼减少术后48小时的恶心呕吐发生率,是值得推荐的防治PONV药物。     

LC-MS法测定人血浆中吡嘧司特钾浓度及药代动力学

目的:建立LC-MS测定人血浆中吡嘧司特钾浓度的方法,测定志愿者口服吡嘧司特钾分散片后的血药浓度,估算其药代动力学参数并对试验制剂与参比制剂的生物等效性进行评价.方法:血浆中加入对乙酰氨基酚为内标,酸化后经二氯甲烷-乙酸乙酯(20∶80)提取,进行LC-MS测定.色谱柱为Shim-pack VP-ODS C18(250 mm×2.0 mm ID),流动相为CH3OH-20 mmol/L NH4Ac,pH 3.0(50∶50),流速0.2 ml/min;ESI选择性正离子检测.临床实验方案采用双交叉实验设计.结果:吡嘧司特钾血浆线性范围为10～1 000 ng/ml,检测限为5 ng/ml.方法回收率大于80%.测定了20名志愿者单剂量交叉口服试验制剂与参比制剂后的血药浓度经时过程,测得试验片与参比片的主要药代动力学参数无显著性差异,试验片的相对生利用度为(99.6±14.6)%.结论:本方法操作简单,专属性强,灵敏度高,准确性好.试验片和参比片生物等效.     

LC-MS和HPLC法测定人血浆中格列本脲和二甲双胍方法的建立

目的建立人血浆中盐酸二甲双胍的高效液相色谱和格列本脲的液相色谱-质谱测定方法.方法二甲双胍血浆样品经乙腈直接沉淀蛋白进样.分析柱:EC 250/4.6 NUCLEOSIL 100-5(4.6mm×250mm,5μm);流动相:0.03 mol/L(NH4)H2P04:乙腈(75:25,pH 7.0),流速1.0 ml/min;检测波长240 nm.格列本脲血浆中加入格列吡嗪为内标,经乙酸乙酯提取,进行LC-MS测定.色谱柱为ORBAX SB300C18柱(2.1 mm×150 mm,5 μm),流动相为乙腈:0.1%乙酸铵(55:45),流速为0.2 ml/min;ESI选择性正离子检测.结果格列本脲浓度为2～200 ng/ml线性关系良好(r=0.999 8),盐酸二甲双胍浓度为6.25～4 000 ng/ml线性关系良好(r=0.999 9).二甲双胍和格列本脲方法的日内和日间RSD＜5%.结论所建立的人血浆中格列本脲的HPLC-MS测定方法和二甲双胍的HPLC测定方法灵敏、准确、简便,可用于格列本脲、二甲双胍的人体药代动力学研究.     

UFLC-MS/MS测定大鼠皮下及血液微透析样品中鬼臼毒素浓度

目的 建立和验证一个测定大鼠皮肤下及血液微透析样品中鬼臼毒素浓度的超高速液相色谱-质谱联用(UFLC-MS/MS)方法.方法 微透析样品中加入依托泊苷为内标,经乙酸乙酯液,液提取后进行UFLC-MS/MS测定.采用Agilent ZORBAX XDB-C18色谱柱(2.1 mmx50mm,3.5μm),柱温为室温,以乙腈-10mmol/L乙酸铵(40:60,V/V)为流动相,流速0.3ml/min;质谱采用正离子模式和多反应离子监测方式进行检测.结果 用于定量分析的离子对分别为m/z432.7→397.3(鬼臼毒素)和589.5→229.5(依托泊苷,内标),鬼臼毒素标准曲线线性范嗣为2.0～1000ng/ml.最低定量下限及最低检测限分别为2.0nedml和0.7 ng/ml.日内和日问精密度及准确度均小于15%.结论 该方法灵敏度高、专属性强,可用于测定大鼠皮肤下及血液微透析样品中鬼臼毒素含量.     

APPLICATION OF LORNOXICAM TO PATIENT-CONTROLLED ANALGESIA IN PATIENTS UNDERGOING ABDOMINAL SURGERIES

FOR anesthesiologis s ,treatingpostoperativepainhas alwaysbeen a problem.Althoughopioidshave been provedtobe effective,theirsideeffectscouldnotbeignored.With thedevelopmentofscienceand pharmacology,many drugs with aspectsof satisfactoryanalgesicefficacyand couldbe welltoleratedby patientshave been developed.And lornoxicamisone of them, which isa non-steroidalanti-inflammatorydrug (NSAID ), with analgesic, anti-infl-ammatory,andantipyreticproperties.Itseliminationhalf-time(3 to 5 hours) isle…     

Dr.Zhang Ren''''s Experience in the Acupuncture Treatment of Different Diseases with the Same Therapeutic Principle

Dr.Zhang Ren,the chief physician,is the chairman of Shanghai Acupuncture and Moxibustion Association.Having been engaged in medicine for about 40 years,he is experienced in treating various intractable diseases.In his long years of clinical practice,he advocates taking the TCM differentiation as the basis to seek for the acupuncture method for treatment of modern intractable diseases.The author of this essay had the fortune to follow Dr.Zhang in study.The following is a summary of Dr.Zhang's experience in the acupuncture treatment for different intractable diseases with the same therapeutic principle.     

Luo Lingjie''''s Experience in Treating Chronic Nephropathy

In treating chronic nephropathy,Luo Lingjie,a chief physician,pays attention to regulating the balance between yin and yang,treating infection if present,and removing pathogenic factors.He prescribes gentle drugs and uses carefully strongly warming-tonifying ones,emphasizes the importance of persuading the patient to persist in treatment with medication and nurse one's health for recuperation,and is good at combined use of TCM and western medicine therapy and brings the merits of various therapies into full play,with obvious theraoeutic effects.     

Acupuncture Combined with Spinal Tui Na for Treatment of Primary Dysmenorrhea in 30 Cases

Objective: To observe the therapeutic effects in acupunture treatment of primary dysmenorrhea combined with spinal Tui Na, and study its mechanism. Methods: Thirty cases of the treatment group were treated by acupuncture combined with spinal Tui Na, and thirty cases in the control group were treated by routine acupuncture. Results: The total effective rate was 93.3% in the treatment group, and 73.3% in the control group, with a significant difference between the two groups (P<0.05). Conclusions: Acupuncture combined with spinal Tui Na has good prospects for treatment of primary dysmenorrhea.     

猪肺磷脂注射液联合经鼻持续气道正压通气对呼吸衰竭早产儿的临床疗效及肌酸激酶同工酶活性的影响

目的 探讨猪肺磷脂注射液联合经鼻持续气道正压通气(NCPAP)对呼吸衰竭早产儿的临床疗效及肌酸激酶同工酶活性(CK-MB)的影响.方法 选取呼吸衰竭早产儿80例,分为观察组和对照组各40例.对照组采用NCPAP给氧治疗,观察组给予NCPAP给氧联合猪肺磷脂气管内给药.观察两组患儿治疗前及治疗12h、24 h后PaO2、PaCO2、血氧饱和度(SaO2)、pH的变化情况,检测治疗前及治疗5d后血清CK-MB水平;评估两组患儿的临床治疗效果.结果 两组患儿PaO2、PaCO2、SaO2、pH比较,差异均有统计学意义(P＜0.05),其中观察组治疗后的PaO2、SaO2、pH均高于对照组,PaCO2则低于对照组.两组的PaO2、SaO2、pH均随观察时间延长而升高(P＜0.05),PaCO2均随观察时间的延长而降低(P＜0.05).观察组治疗有效率为87.5％,显著高于对照组的70.0％ (P ＜0.05).治疗5d后两组患儿血清CK-MB水平均较前降低(P＜0.05),且观察组明显低于对照组(P＜0.05).结论 猪肺磷脂注射液气管内给药联合NCPAP可以显著降低呼吸衰竭早产儿CK-MB的含量,提高治疗有效率,起到很好的呼吸循环支持作用.     

Survey and practice of reporting quality of randomized controlled clinical trials on traditional Chinese medicine

Evidence obtained from randomized controlled trials （RCTs） has been generally accepted as the gold standard in the evaluation of clinical effectiveness. Readers need to understand the trial design, implementation, results, analysis and interpretation, so as to fully Jnderstand the results of RCTs. Thus, the investigators of RCTs have to report these items in a complete, accurate and clear manner. Since 1998, we have conducted several evaluations on the reporting quality of RCTs published in Chinese journals on traditional Chinese medicine （TCM） and results have shown that there is an urgent need for higher quality RCTs on TCM.     

TCM Treatment of Ankylosing Spondylitis by Tonifying the Kidney and Strengthening the Governor Vessel

Ankylosing spondylitis is a chronic and progressive disorder with inflammation mainly involving the central axis joints. It mainly affects the cervical spine and the lumbosacral area, with the pathogenesis closely related to the kidney and the Governor Vessel (GV). TCM holds that the syndrome is deficiency in origin and excess in superficiality, which is due to insufficiency of the kidney, deficiency of GV, and blocking of the channels with the invasion of exogenous evil, leading to poor circulation of qi and blood and malnutrition of the bones, muscles and joints. The TCM method of tonifying the kidney and strengthening GV to regulate circulation of qi and blood and check the arthralgia pain should be adopted, with the Kidney-Tonifying and GV Strengthening Decoction (益肾强督汤) prescribed.     

IMPROVING P-gp EXPRESSION IN HUMAN MONONUCLEAR CELLS IN VITRO TRANSFECTED BY MULTIDRUG RESISTANCE-1 mRNA

CHEMOTHERAPY playsa greatrolein the treat- ment of malignanttumors,especiallyingynecolo- gicalones.But inanticancerchemotherapy,leuko-cytopeniaisfrequentlytheprimarydose-limitingsideeffect factor.Moreover,cancersarefrequentlychemoresistantbe-causeof overexpressionof P-glycoprotein(P-gp), which isencodedby multidrugresistancegene (MDR1 ) and detectableinup to50% ofhuman cancersand renderscellsresistancetoanticancerdrugs.The safetyand potentialtherapeuticbenefitof mdr1 gene transferredto h…